反应详情

温度

40 °C

To a mixture of compound 11 (0.137 mmol), compound 3a (0.206 mmol), and HATU (0.206 mmol) in dimethylformamide (1.5 mL) was added TEA (0.55 mmol) dropwise. The reaction mixture was stirred at 40° C. for 4 hrs. The solvent was removed under reduced pressure and the residue dissolved in a mixture of dichloromethane/methanol (9/1). This mixture was passed through a SCX-2 column and the column was washed three times with the same eluent. The filtrate was concentrated and the residue was purified by chromatography on a silica gel column to give compound 12a as a yellow orange solid in 18% yield. MS (ESI, EI+) m/z=548.24-550.20 (MH+).

1. customThe solvent was removed under reduced pressure
2. dissolutionthe residue dissolved in a mixture of dichloromethane/methanol (9/1)
3. washthe column was washed three times with the same eluent
4. concentrationThe filtrate was concentrated
5. customthe residue was purified by chromatography on a silica gel column